Method for deacidifying alpha-ethylli-nolenate solvent

A technology of ethyl linolenate, esterification and deacidification, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of low esterification rate, large amount of solvent and acidic catalyst, and achieve The effect of reducing acid value, reducing consumption and reducing discharge

Inactive Publication Date: 2012-07-18
河北欣奇典生物科技有限公司
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of this invention is to provide a method for solvent deacidification of ethyl α-linolenic acid, to solve the shortcomings of low esterification rate in the traditional direct esterification deacidification process, large amount of solvent and acidic catalyst, improve the yield, cut costs

Method used

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  • Method for deacidifying alpha-ethylli-nolenate solvent

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Put 1000kg of α-ethyl linolenic acid with an acid value of 8 and 2000 kg of ethanol with a concentration of 80% into the reaction kettle, stir and mix evenly, let stand for 30 minutes, put the lower layer (α-linolenic acid ethyl ester layer) into the distillation In the kettle, distill under reduced pressure, reclaim ethanol, remove moisture to a moisture content of ≤0.1%, obtain 950 kg of ethyl α-linolenic acid product, and detect an acid value of 0.48;

[0031] Add 1 kg of concentrated sulfuric acid to the upper layer (free acid layer), heat up to 85°C, reflux for 6 hours, cool down to 30°C, wash with saturated brine until neutral, dehydrate under reduced pressure to 0.1% moisture, and obtain ethyl α-linolenic acid product 49.3kg, the detected acid value is 0.88.

Embodiment 2

[0033] Put 1000 kg of α-ethyl linolenic acid with an acid value of 8 and 500 kg of ethanol with a concentration of 95% into the reaction kettle, stir and mix evenly, let stand for 180 minutes, put the lower layer (α-linolenic acid ethyl ester layer) into the distillation In the kettle, distill under reduced pressure, reclaim ethanol, remove moisture until the moisture is 0.05%, and obtain 810kg of ethyl α-linolenic acid product, and the detected acid value is 0.26;

[0034] Add 5.7kg of concentrated sulfuric acid to the upper layer (free acid layer), heat up to 76°C, reflux for 1 hour, cool down to 35°C, wash with saturated brine until neutral, dehydrate under reduced pressure until the water content is 0.07%, and obtain α-linolenic acid ethyl The ester product was 189.3kg, and the detected acid value was 0.99.

Embodiment 3

[0036] Put 1000kg of α-linolenic acid ethyl ester with an acid value of 8 and 1000kg of ethanol with a concentration of 90% into the reaction kettle, stir and mix evenly, let stand for 90 minutes, put the lower layer (α-linolenic acid ethyl ester layer) into the distillation In the kettle, distill under reduced pressure, reclaim ethanol, remove moisture until the moisture is 0.08%, obtain 880kg of ethyl α-linolenic acid product, and detect the acid value as 0.35;

[0037] Add 3kg of sulfonic acid to the upper layer (free acid layer), raise the temperature to 80°C, reflux for 4h, wash with saturated brine until neutral, dehydrate under reduced pressure until the water content is 0.08%, and obtain 119.6kg of ethyl α-linolenic acid product. The acid value is 0.90.

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Abstract

The invention relates to a method for deacidifying an alpha-ethylli-nolenate solvent. The method comprises the following steps of: mixing alpha-ethylli-nolenate with a high acid value and ethanol, standing and layering until two systems are separated, concentrating and dealcoholizing the lower alpha-ethylli-nolenate layer by the conventional mode, and esterifying and deacidifying the upper free acid layer, wherein ethanol is edible ethanol at the concentration of 80 to 95 percent, and the mixing ratio of alpha-ethylli-nolenate to ethanol is 1:(0.5-2). By the method, the acid value of a product can be effectively reduced, the defects of low esterification rate, and large using amount of solvent and acid catalyst and the like in the conventional direct esterifying and deacidifying process are overcome, production cost is reduced, and the alpha-ethylli-nolenate solvent is easy to prepare and convenient to produce and use, and can be industrially produced conveniently.

Description

technical field [0001] The invention relates to a method for deacidifying unsaturated fatty acid esters, in particular to a method for solvent deacidifying ethyl α-linolenic acid. Background technique [0002] At present, the country has no relevant national standards for the acid value of α-linolenic acid / α-linolenic acid ethyl ester. The national standard for linseed oil (GB / T 8235-2008) is used, and the first-grade pressed linseed oil is used in the standard. The acid value of linseed oil is 1.0 (calculated by KOH) mg / g, and the acid value of second-stage pressed linseed oil is 3.0 (calculated by KOH) mg / g. However, in the process of producing α-linolenic acid ethyl ester with linseed oil as raw material, since the raw material needs to be processed by transesterification, water washing, dehydration, etc., during the processing, the raw material needs to be treated with water, heating, stirring, etc., which is very easy to cause α-Ethyl linolenic acid is hydrolyzed into ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/587C07C67/60
Inventor 王小锋余海龙李旭明
Owner 河北欣奇典生物科技有限公司
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